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Dimethyl Sulfoxide → 3-Methyl-11-(4-methyl-piperazin-1-yl)-3-methyl-5H-dibenzo[b,e][1,4]diazepine

HRID 1350509
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HRID 1350509 반응식
Cl.[CH3:2][C:3]1[CH:4]=[CH:5][C:6]2[C:12]([NH2:13])=[N:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[NH:8][C:7]=2[CH:18]=1.[CH3:19][N:20]1[CH2:25][CH2:24]N[CH2:22][CH2:21]1.[CH:26](N(CC)C(C)C)(C)C.CS(C)=O>Cl.C(OCC)(=O)C.C1(C)C=CC=CC=1>[CH3:2][C:3]1([CH3:26])[CH:18]=[C:7]2[NH:8][C:9]3[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=3[N:11]=[C:12]([N:13]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[C:6]2=[CH:5][CH2:4]1
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8

반응물 4

HCID 679Dimethyl SulfoxideHCID 531671-MethylpiperazineHCID 81531DiisopropylethylamineHCID 210935233-Methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride

생성물 1

HCID 694899693-Methyl-11-(4-methyl-piperazin-1-yl)-3-methyl-5H-dibenzo[b,e][1,4]diazepine수율 42%

시약·촉매·용매 3

HCID 313
Hydrochloric Acid
촉매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

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온도
110 °C

실험 절차

Combine 3-methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride (636.4 mg, 2.85 mmol), N-methylpiperazine (444.2 mg, 3.08 mmol), N,N-diisopropylethylamine (856.5 mg, 8.55 mmol), DMSO (2.0 ml), and toluene (4.0 ml). Stir and heat the mixture at 110° C. After 48 hours, add one drop of 5N HCl. After 72 hours, cool the mixture to ambient temperature and then dilute it with ethyl acetate. Wash the organic layer with DI H2O and brine. Dry (sodium sulfate) and concentrate the organic layer to residue. Purify the residue on silica gel using dichloromethane/methanol (90:10) to give 362.9 mg (42%) of a tan foam: mp 84°, dec; mass spectrum (ion spray): m/z=307.1 (M+1).

후처리

  1. waitAfter 72 hours
  2. temperaturecool the mixture to ambient temperature
  3. washWash the organic layer with DI H2O and brine
  4. dry with materialDry (sodium sulfate)
  5. concentrationconcentrate the organic layer to residue
  6. customPurify the residue on silica gel

출처 및 근거

ORD 기록
ord-21e08f58f120417ab45618e4052d5917
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214673B2

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